US20170252668A1 - Distillation and rotary evaporation apparatuses, devices and systems - Google Patents

Abstract

Provided herein are integrated distillation apparatuses configured as stand-alone fully integrated systems having a reduced footprint. Integrated distillation apparatuses can have a rotary evaporator, a condenser, and an integrated refrigeration system or chiller, as well as an integrated water bath and vacuum pump, all of which can be integrated into a central frame and/or housing assembly. Integrated distillation apparatuses can be configured such that the rotary evaporator is movably attached to a frame structure and configured to be vertically translatable in position, whereas the condenser can be affixed to the structure by an arm extending from the structure and adjacent to the rotary evaporator, and wherein the refrigeration system can be in fluid communication with the condenser.

Description

CROSS REFERENCE TO RELATED APPLICATIONS
• This application claims the benefit of and priority to U.S. Provisional Patent Application Ser. No. 62/084,097, filed Nov. 25, 2014, and the benefit of and priority to U.S. Provisional Patent Application Ser. No. 62/109,993, filed Jan. 30, 2015, the disclosures of which are incorporated herein by reference in their entireties.
TECHNICAL FIELD
• The presently disclosed subject matter relates to distillation and rotary evaporation apparatuses, devices and systems. The presently disclosed subject matter also relates to the use of such distillation and rotary evaporation apparatuses, devices and systems.
BACKGROUND
• Rotary evaporators, also referred to as distillers, are used in laboratories throughout the world, for removing solvents from organic and inorganic solutions, to yield a liquid or solid product. Generally, such evaporators or distillers work by evaporating a solvent and then condensing the evaporate into a collection vessel. Such evaporators, while functional, have limitations and inefficiencies that need to be addressed.
• What are needed are rotary evaporator designs and systems that provide sufficient cooling and condensing capabilities that are cost effective and easy to use. Additionally, rotary evaporator designs that are fully integrated and easier to use are needed, particularly where improved yield and efficiencies can be realized. Additionally, rotary evaporator designs that are compact and have a small footprint are needed. Such advantages, and others disclosed herein, are provided by the instant disclosure.
SUMMARY
• The presently disclosed subject matter provides integrated and stand-alone distillation and rotary evaporation apparatuses, devices and systems configured to operate efficiently while taking up less space. That is, distillation apparatus as provided herein can comprise a fully integrated unitary distillation apparatus and/or rotary evaporator configured with all components required for operation in a compact design, including in some embodiments integrated mechanical cooling/refrigeration systems.
• An object of the presently disclosed subject matter having been stated hereinabove, and which is achieved in whole or in part by the presently disclosed subject matter, other objects will become evident as the description proceeds when taken in connection with the accompanying Examples as best described hereinbelow.
BRIEF DESCRIPTION OF THE DRAWINGS
• The presently disclosed subject matter can be better understood by referring to the following figures. The components in the figures are not necessarily to scale, emphasis instead being placed upon illustrating the principles of the presently disclosed subject matter (often schematically). In the figures, like reference numerals designate corresponding parts throughout the different views. A further understanding of the presently disclosed subject matter can be obtained by reference to an embodiment set forth in the illustrations of the accompanying drawings. Although the illustrated embodiment is merely exemplary of systems for carrying out the presently disclosed subject matter, both the organization and method of operation of the presently disclosed subject matter, in general, together with further objectives and advantages thereof, may be more easily understood by reference to the drawings and the following description. The drawings are not intended to limit the scope of this presently disclosed subject matter, which is set forth with particularity in the claims as appended or as subsequently amended, but merely to clarify and exemplify the presently disclosed subject matter.
• For a more complete understanding of the presently disclosed subject matter, reference is now made to the following drawings in which:
• FIGS. 1A and 1B are perspective views of two embodiments of distillation apparatuses as disclosed herein;
• FIGS. 2A through 2E are schematic illustrations of components of a condenser configured to be used in the disclosed distillation apparatuses;
• FIG. 3 is a cross-sectional view of a distillation apparatus as disclosed herein;
• FIG. 4 is a perspective view of an embodiment of a distillation apparatus as disclosed herein;
• FIG. 5 is a schematic illustration of the operation of a distillation apparatus as disclosed herein;
• FIGS. 6A and 6B are perspective views of two embodiments of distillation apparatuses as disclosed herein;
• FIGS. 7A and 7B are perspective views of two embodiments of distillation apparatuses as disclosed herein;
• FIGS. 8A and 8B are perspective views of two embodiments of distillation apparatuses as disclosed herein;
• FIGS. 9A through 9C are illustrations of a rotary evaporator assembly, including an exploded or component view (FIG. 9A), a partial assembled view (FIG. 9B), and fully assembled view (FIG. 9C); and
• FIG. 10 is a perspective view of an embodiment of a distillation apparatus as disclosed herein.
DETAILED DESCRIPTION
• Rotary evaporators, also referred to in some embodiments as distillers or distillation apparatuses, are used in laboratories throughout the world, for removing solvents from organic and inorganic solutions, to yield a liquid or solid product. Generally, such evaporators or distillers work by placing a sample in a round-bottom flask (referred to as a sample flask or evaporation flask), typically a pear-shaped flask, which spins on an axis at an angle while sitting in a water bath. The flask is attached to a motor, which can include a rotary joint that enables the flask to spin, while permitting the evaporated solvent to flow through the joint (vapor duct) and come into contact with one or more condensers. The condenser(s) can cool the vapor, and the resulting cooled vapor (i.e., liquid) then flows down to a flask below the condenser (a collection flask), where it can be collected.
• A water bath can typically be provided to supply sufficient heat to the flask to evaporate the solvent. Typically, the rotor, the motor, the rotary joint, the condenser, the flask used to hold the original solvent, and the flask used to hold the condensed vapor as it is collected, are all connected while the unit is in operation. A mechanical arm is usually provided to raise and lower the connected parts, to bring the flask out of the water bath.
• The condenser of the rotary evaporator can be connected to a water source, and water is frequently acceptable to condense the solvent of interest, particularly if the solvent has a relatively high boiling point. Users frequently leave the water flowing through the condenser throughout the day, which results in large volumes of waste water. Further, where the solvent has a particularly low boiling point, it can be advantageous to cool the vapor to temperatures cooler than a water condenser can provide. To only use a water-cooled condenser might create an environmental issue, as a significant volume of volatile organic solvent would not be collected, and could instead enter into the environment.
• Particularly when low boiling solvents are used, efforts have been made to improve on the condensation of the vapors so as to trap a significant portion of the solvents. In such cases, one approach is to use a dry-ice condenser, which is packed with dry ice, and, optionally, a solvent that forms a slurry with dry ice to maintain a given temperature (for example, dry ice-acetone maintains a temperature of −78° C.). However, since glass is a poor conductor of heat, the “cold finger” glass of the dry-ice condenser provides warmer than −78° C. cooling surface on which vapors are condensed. Also, in normal laboratory operating temperatures (ambient) dry ice evaporates very fast, which requires constant or frequent replenishing of dry ice in the dry-ice condenser. This is costly, burdensome and negatively impacts productivity.
• Provided herein are distillation apparatuses, also referred to as rotary evaporators, rotary distillers, distillers, evaporators, and the like. More particularly, provided herein are distillation apparatuses configured as all-in-one or stand alone distillation apparatus, and configured in a compact design. That is, a distillation apparatus as provided herein can comprise a fully integrated unitary distillation apparatus and/or rotary evaporator configured with all components required for operation in a compact design.
• Distillation apparatuses provided herein can in some embodiments comprise integrated cooling systems, such as for example a refrigerated condensing unit. Thus, in some embodiments disclosed rotary evaporators and/or distillation apparatuses can be capable of cooling evaporated solvents without using a dry ice trap, a continuous flow of water, and/or a recirculating chiller. By using a mechanically refrigerated cooling/freezing system, or chiller, to provide a cool reservoir capable of condensing vapors arising from solvent evaporation the waste of a continuous flow of water can be avoided, and the use of dry ice and compatible solvents such as acetone and isopropyl alcohol can be avoided, both of which provide for a more environmentally friendly alternative to existing rotary evaporators. Moreover, the configuration and design of the disclosed rotary evaporator and/or distillation apparatuses provides for the use of refrigeration cooling/heat exchange system in an integrated and compact design, particularly as compared to existing evaporators that comprise multiple components and require substantially more space to operate.
• A rotary evaporator can in some aspects comprise a sample container, such as a sample flask, which is rotated integrally with a rotary joint. The sample flask can be soaked within a water bath, in some embodiments a heated water bath. The sample flask can be connected to one end of the rotary joint through a vapor duct that can be insertedly supported by a rotor of a motor through a sleeve. On the other side of the rotary joint there can in some embodiments be one or more condensers connected by a vapor duct to receive and thereby condense vapors evaporated from the sample flask.
• In some embodiments a main body of the motor can be structured by a stator and a motor housing. As the motor is engaged, for example by supplying a current to the motor, a rotational force can be applied to the sample flask within the water bath through the rotary joint. In some embodiments the rotary joint can be insertedly supported by the sleeve in an insertion area. The sleeve can be fixed in engagement with the motor rotor. Furthermore, the sleeve can be rotatably supported by the motor main body at both ends thereof by bearings or the like. In some aspects a fastening member can be arranged within the sleeve for engaging and fastening the rotary joint (vapor duct) to the sleeve. The fastening member can comprise a fastening cap engaged with the sleeve. In some aspects the a coupling member can comprise a plurality of bushes slidably mounted on the outer peripheral surface of the rotary joint and an elastically deformable O-ring disposed between the bushes so that the O-ring can be pressured by the fastening force through the bushes such that the O-rings can be tightly contacted to the outer peripheral surface of the rotary joint and to the inner surface of the sleeve by elastic deformation. An air tight seal can be created at the junction of the rotary joint and rotational motor.
• The rotation of the motor rotor can be transmitted to the rotary joint to rotate the rotary joint and thereby rotate the sample container or sample flask. Where the sample flask is at least partially submerged within the water heated water bath the sample can be evaporated and steam or vapor generated within the sample container. This evaporate can then pass through the rotary joint (vapor duct) and to the condenser.
• Once at the condenser the evaporate or vapor can come into contact with a cooled surface, such as for example a heat exchanger, to thereby cause the evaporate or vapor to cool and condense into a liquid. Once in liquid form the condensed sample drips or falls by way of gravity into a collection flask positioned below the condenser. In some aspects the condenser can comprise a joint or other conduit to connect the condenser to a collection flask. The condenser can in some embodiments also comprise a port, tube or hose configured to connect the condenser to a vacuum line, such that the sample or solvent of interest can be evaporated under vacuum. The vacuum can in some embodiments be applied near the top of the condenser to provide the maximum opportunity for the vapor to be cooled, thus minimizing the opportunity that solvent vapors will pass on to the vacuum system, such as to the vacuum pump or vacuum trap.
• In some embodiments, the distillation apparatus comprises a chiller mechanically connected to a condenser comprising a heat exchanger. The chiller can comprise a refrigeration system, including refrigeration lines, such as copper lines, through which refrigerant can pass, and a receiving tank, compressor, refrigeration condenser and dryer. The refrigeration lines can be connected to a heat exchanger in the condenser unit that cools the evaporate. In some embodiments a cooling coil, which can be exposed, or in some embodiments concealed in a chemically-resistant vapor trap or sleeve made of titanium (including commercial pure grade titanium), stainless steel, metal alloys, plastic, glass, rubber, such as neoprene rubber, and/or combinations thereof, can be fluidly connected to the refrigeration lines. In some embodiments titanium is used in the sleeve due to its robust chemical resistance. The condenser unit in some embodiments can comprise a cooling coil chamber that is cooled by direct expansion of refrigerant in the refrigeration lines. In some embodiments, the heat exchanger can comprise a copper coil through which cooled refrigerant passes, and which is encased in a titanium sleeve. In some embodiments, the heat exchanger can comprise a coil that is double looped and not encased in a sleeve such that vapors are exposed to an increase surface area on the cooled coils. In such embodiments the double coils can comprise stainless steel, titanium, and/or a combination thereof. In some embodiments, the chiller, including mechanical refrigeration system, can be mechanically linked to and fixed with the heat exchanger/condenser such that the two are provided in a single unitary device.
• In some embodiments a distillation apparatus as disclosed herein can comprise a mounting arm configured to hold and position a rotary evaporator assembly such that the rotary evaporator assembly is an integrated component of the distillation apparatus along with the chiller and condenser. Such a mounting arm can comprise a rotor, motor, and/or rotary joint configured to rotatably support and engage a vapor tube, with a sample flask at one end. The opposing end of the vapor tube can engage a dummy condenser or cooling condenser unit. In some aspects the mounting arm is configured to support and facilitate the operation and functionality of the rotary evaporator assembly and integrate it into the unitary distillation apparatus. In some embodiments the mounting arm is mechanically linked to a main frame of the distillation apparatus, including in some embodiments a vertically adjustable member that is configured to allow the mounting arm, and attached rotary evaporator assembly, to raise and lower vertically as need to optimally position the sample flask in a water bath. In some embodiments the vertically adjustable member comprises a motorized member configured to move the mounting arm along a track or other guiding component to thereby raise and lower the mounting arm. The track or guiding component can in some embodiments be integrated into a portion of the main frame or housing of the chiller.
• In one embodiment, a distillation apparatus as disclosed herein can further comprise an adjustable platform underneath and/or integrated into the water bath to raise and lower the bath relative to the collection flask. In some aspects the adjustable water bath can be motorized such that the vertical and/or horizontal positioning of the water bath can be adjusted. Thus, in some embodiments where the positioning of the water bath is adjustable the rotary evaporator itself, and the condenser attached to the rotary evaporator, can remain in a fixed position. In some aspects the water bath can weigh significantly less than the remainder of the device, such that moving the water bath is easier than raising and lowering the rotary evaporator.
• Thus, in some embodiments an integrated distillation apparatus is provided herein, comprising a rotary evaporator configured to evaporate a sample, a condenser configured to condense an evaporated sample, a refrigeration system configured to cool the condenser, a collection vessel configured to collect a condensate, and a vacuum pump configured to create a vacuum in the evaporator, wherein each of the components is integrated into a single apparatus. Moreover, in some embodiments, the integrated distillation apparatus can further comprise a motorized component configured to provide a rotational force, a rotary joint insertedly supported within the motorized component upon which the rotational force is applied, a sample container connected to a first end of the rotary joint, a water bath into which the sample container can be placed, wherein the water bath is configured to provide heat energy to the sample container, a condenser connected to a second end of the rotary joint, wherein the condenser is configured to receive a collection flask that receives condensed vapors condensed off of the condenser, and a cooling coil configured to engage the condenser, wherein the cooling coil is configured to receive coolant from the refrigeration system, whereby the condenser is sufficiently cool to condense vapors coming into contact with the condenser. In some embodiments an integrated distillation apparatus as disclosed herein can further comprise a mechanical linkage configured to move the water bath in a vertical and/or horizontal direction to engage the sample container.
• In some embodiments the refrigeration system can comprise a condenser and refrigerant, wherein the refrigeration system provides coolant to the condenser to thereby condense vapors from the evaporator. In some embodiments the coolant is provided to a double coil inside the condenser, wherein the vapors come into contact with the double cool or a wall surrounding the double coil. The refrigeration system can be configured to cool the condenser from about ambient temperature to about −100° C.
• In some embodiments an integrated distillation apparatus as disclosed herein can further comprise a frame configured to integrate all components into a single apparatus, wherein the water bath is configured to move relative to the rotary evaporator, wherein the rotary evaporator, refrigeration system, collection vessel, condenser and vacuum pump are stationary within the frame. The collection vessel can comprise a first and second compartment divided by a vacuum valve, wherein the first compartment can be removed to collect the condensate while the vacuum valve preserves the vacuum on the evaporator and the second compartment continues to collect condensate. The condenser can comprise two or more condensers in a series.
• In some embodiments an integrated distillation apparatus as disclosed herein can further comprise a vacuum seal inside the condenser. The vacuum seal inside the condenser can comprise an O-ring incorporated inside the condenser at a point where the rotary evaporator engages the condenser. The O-ring can provide an internal vacuum seal.
• In some embodiments an integrated distillation apparatus as disclosed herein can further comprise a collapsible member disposed between the condenser and rotary evaporator, whereby the collapsible member is configured to allow an adjustment in the positioning of the rotary evaporator while connected to the condenser.
• In some embodiments an integrated distillation apparatus as disclosed herein can further comprise a frame structure configured to house the refrigeration system and vacuum pump, and structurally support the rotary evaporator and condenser. The frame structure can be configured to support the condenser in a fixed position while supporting the rotary evaporator in a movable position.
• In some embodiments provided herein is an integrated distillation apparatus comprising a rotary evaporator configured to evaporate a sample, a condenser configured to condense an evaporated sample, and a refrigeration system configured to cool the condenser, wherein the rotary evaporator, condenser and refrigeration system are integrated into a single structure, wherein the rotary evaporator is movably attached to the structure and configured to be vertically translatable in position, wherein the condenser is affixed to the structure by an arm extending from the structure and adjacent to the rotary evaporator, and wherein the refrigeration system is in fluid communication with the condenser. In some embodiments an integrated distillation apparatus as disclosed herein can further comprise a motorized component configured to provide a rotational force to the rotary evaporator. In some embodiments an integrated distillation apparatus as disclosed herein can further comprise a mechanical linkage to vertically translate the position of the rotary evaporator. In some embodiments an integrated distillation apparatus as disclosed herein can further comprise a heated water bath into which a sample container of the rotary evaporator can be submerged.
• In some embodiments the condenser can comprise a cooling coil in fluid communication with the refrigeration system. The condenser can comprise a titanium sleeve surrounding the cooling coil, whereby the titanium sleeve is cooled by the cooling coil, wherein an evaporate from the rotary evaporator comes into contact with the titanium sleeve and condenses. The condenser can comprise metal alloy sleeve surrounding the cooling coil, whereby the metal alloy sleeve is cooled by the cooling coil, wherein an evaporate from the rotary evaporator comes into contact with the metal alloy sleeve and condenses.
• Turning now to the figures, two embodiments of an integrated all-in-one distillation apparatus as provided herein are illustrated inFIGS. 1A and 1B. As depicted inFIGS. 1A and 1B, fully integrated all-in-onedistillation apparatus100 and102, respectively, can comprise achiller120, arotary evaporator assembly140 and acondenser180. In some embodiments, and as shown inFIGS. 1A and 1B, thechiller120,rotary evaporator assembly140, and acondenser180, can be integrated into a single device or apparatus that is configured to compactly arrange the elements in such a way that provides for an effective and efficient distillation system while minimizing the operational area and/or footprint. For example, the footprint or operational area ofdistillation apparatus100 and102 can be defined by the length L, width W, and/or combination thereof (area in square inches for example) of the outer dimensions of the apparatus. Alternatively, or in addition, the footprint or operational area ofdistillation apparatus100 and102 can be defined by the length X, width Y, and/or combination thereof (area in square inches for example) of the dimensions of the base or platform of the housing/frame.
• Continuing withFIG. 1A,distillation apparatus100 can comprise achiller120.Chiller120 can comprise in some embodiments alower housing122 andupper housing126, withupper housing126 extending substantially vertically fromlower housing122. In someembodiments chiller120 can comprise acondenser arm124 extending substantially horizontally fromupper housing126 and configured to support and mechanically connectcondenser180 tochiller120.Chiller120 can comprise an integrated refrigeration system (seeFIG. 3) housed withinlower housing122 andupper housing126, and continuing throughcondenser arm124 to provide a cooled refrigerant tocool condenser180. In some embodiments,lower housing122 can house components of a refrigeration system (solely or in conjunction with upper housing126), such as for example a receiving tank, compressor, refrigeration condenser and dryer (seeFIG. 3), all or some of which can bee connected by refrigeration lines (copper tubing) tocondenser180 by feeding throughupper housing126 andcondenser arm124. In some embodimentslower housing122 can comprise ventilation grates194 configured to allow airflow intohousing122 and around the refrigeration system housed therein.
• Mountingarm154 can be mechanically linked to and can extend (substantially horizontally in some embodiments) fromupper housing126. Mountingarm154 can be configured to support, hold and/or positionrotary evaporator assembly140 such thatrotary evaporator assembly140 is an integrated component, or can become an integrated component by mounting to mountingarm154, ofdistillation apparatus100, along withchiller120 andcondenser180. In someembodiments mounting arm154 can be mechanically linked toupper housing126 by a verticallyadjustable member160 that is configured to allow mountingarm154, and attachedrotary evaporator assembly140, to raise and lower vertically as need to optimally position the sample flask in a water bath. In some embodiments verticallyadjustable member160 can comprise a motorized member configured to move mountingarm154 along a track or other guiding component to thereby raise and lower mountingarm154. The track or guiding component of verticallyadjustable member160 can in some embodiments be integrated into a portion of the main frame or housing of the chiller, such as for exampleupper housing126.
• Rotaryevaporator assembly140 can comprise a rotary joint (vapor duct)150 with asample flask142 at one end, wherebysample flask142 can be rotated integrally with rotary joint150.Sample flask142 can be soaked, bathed or immersed withinwater bath156, in some embodiments a heated water bath to cause evaporation of the sample or solvent insample flask142.Water bath156 can comprise a heating element and controller or other configuration for heating water or other liquid/fluid contained therein.Sample flask142 can be connected to one end of rotary joint150 through opening324 (and in some embodiments secured by clip322), wherein the vapor duct can be insertedly supported by a rotor of a motor through a sleeve housed within mountingarm154. Vapor duct/rotary joint150 can act both as the axis for sample rotation, and as vacuum-tight conduit for the vapor being drawn off of the sample. On the other side of rotary joint150 there can in some embodiments be one or more condensers (condenser180 and/or dummy condenser144) connected byvapor duct150 to receive and thereby condense vapors evaporated fromsample flask142. In someembodiments dummy condenser144 can be used, and can comprise anupper portion146 andlower portion148, as well as aconnector arm328 secured to mountingarm154 and through which rotary joint150 passes intoupper portion146.
• Continuing withFIG. 1A, an evaporating (sample) flask142 can be immersed in awater bath156. Evaporatingflask142 can be rotated using a motor housed in mountingarm154, with the rotational force provided by the motor being transferred to evaporatingflask142 by rotary joint (vapor duct)150. Rotary joint150 can pass/continue through mountingarm154. Rotary joint150 provides a conduit through which the evaporate (vapor) from a sample or solvent inevaporation flask142 can pass into acondenser180 attached to or in communication withvapor duct150.
• Once incondenser180 vapors can be cooled thereby causing them to re-condense and drop intocollection flask186 by way ofconduit158.Collection flask186 can in some embodiments be removed by a releasable joint192, which can in some embodiments comprise a valve to maintain the vacuum incondenser180 and/orrotary evaporator140 untilcollection flask186 is reattached. After the solvent has been removed (by evaporation), evaporatingflask142 can be removed fromwater bath156 by raising mountingarm154 by way of verticallyadjustable member160, which in some embodiments can comprise a track and motor or other mechanized unit.
• Continuing withFIG. 1A,water bath156 can be arranged on top oflower housing122 and adjacent toupper housing126. Such a configuration can minimize the footprint ofdistillation apparatus100, particularly as compared to a distillation system where a water bath is not integrated and is instead placed or arranged on a surface adjacent to the distillation apparatus. Moreover, mountingarm154 arranged onupper housing126 and being vertically adjustable allows forrotary evaporating assembly140 to be raised and lowered such thatsample flask142 can be placed into or removed fromwater bath156 without having to movewater bath156. By vertically orienting these components the overall footprint of the all-in-oneintegrated distillation apparatus100 is greatly reduced, particularly as compared to non-integrated systems.
• Condenser180 can be attached tocondenser arm124 byclamp196, or other attachment mechanism, e.g. threads, screws, bolts, pressure fitting, etc.Condenser180 can comprisecondenser coil182,condenser sleeve198 andcondenser housing184.Condenser coil182 can be configured to fit or slide insidecondenser sleeve198 to form a heat exchanger or “cold finger”.Condenser coil182 can in some embodiments be double looped to increase the surface area for cooling and heat exchange.Condenser coil182 can be fluidly connected to the integrated refrigeration system inchiller120 such that cooled refrigerant passing throughcondenser coil182 causes a cooling effect oncondenser sleeve198. Evaporate or vapor fromrotary evaporator140 enteringcondenser housing184 can come into contact with the cold surface ofcondenser sleeve198 thereby causing the vapor to condense into a liquid to be collected incollection flask186. The configuration ofcondenser180 provides an efficient mechanism for trapping all or substantially all vapors and condensing them such that environmental impacts are lessened.
• In someembodiments condenser coil182 can comprise coiled copper line that forms a continuous loop thereby providing for a continuous flow of a refrigerant material or compound to flow from the heat exchanger incondenser180 to the mechanical refrigeration system inchiller120. While in someembodiments condenser coil182 can be exposed for direct cooling of evaporate (vapor), as depicted inFIG. 1A it can be concealed bycondenser sleeve198 that can comprise a chemically-resistant vapor trap made of titanium (including commercial pure grade titanium), stainless steel, metal alloys, plastic, glass, rubber, such as neoprene rubber, and/or combinations thereof. In some embodiments, the heat exchanger can comprise acoil182 that is double looped and not encased in asleeve198 such that vapors are exposed to an increased surface area on the cooled coils. In such embodiments the double coils can comprise stainless steel, titanium, and/or a combination thereof. As depicted inFIG. 1A, and in order to achieve a stand alone fully integrated system that minimizes space utilization,chiller120, including mechanical refrigeration system, can be mechanically linked to and fixed with the heat exchanger/condenser180 such that the two are provided in a single unitary device.
• Condenser housing184 can comprise a glass vessel enclosing the heat exchanger that includescondenser coil182 andcondenser sleeve198.Condenser housing184 can attach tocondenser arm124 byclamp196 to create an air-tight seal.Condenser housing184 can comprise anentry port188 for receiving an evaporate or vapor fromrotary evaporator assembly140, and in some embodiments asecond entry port188′. Avacuum port190 can in some embodiments be provided (in some cases near the top) and configured to receive a vacuum line from a vacuum pump to thereby cause a vacuum on the inner environment ofcondenser housing184. In some embodiments a vacuum system, including vacuum pump and controller, can be provided indistillation apparatus100, including for example inlower housing120, to reduce the pressure within the evaporator system. An evaporate or vapor that comes into contact withheat exchanger198 incondenser180 and thereby condenses into a liquid can collect intocollection flask186 by passing throughconduit158. In some embodiments a joint192 can be positioned onconduit158 that can be configured to allow for removal of a collection flask (receiving flask)186 without breaking a vacuum to the system during operation. Such joint192 can comprise a valve to maintain the vacuum while removingcollection flask186.
• Turning now to theFIG. 1B,distillation apparatus102 can comprise achiller120.Chiller120 can comprise in some embodiments amain housing132, optionally supported onplatform170. In someembodiments chiller120 can comprise acondenser arm134 extending substantially horizontally frommain housing132, in some embodiments from an upper portion ofmain housing132, and configured to support and mechanically connectcondenser180 tochiller120.Chiller120 can comprise an integrated refrigeration system (seeFIG. 3) housed withinmain housing132 and continuing throughcondenser arm124 to provide a cooled refrigerant tocool condenser180. In some embodiments,main housing132 can house components of a refrigeration system (solely or in conjunction with condenser arm134), such as for example a receiving tank, compressor, refrigeration condenser and dryer (seeFIG. 3), all or some of which can bee connected by refrigeration lines (copper tubing) tocondenser180 by feeding throughcondenser arm134. In some embodimentsmain housing132 can comprise ventilation grates194 configured to allow airflow intohousing132 and around the refrigeration system housed therein.
• Mountingarm154 can be mechanically linked to and can extend (substantially horizontally in some embodiments) frommain housing132. Mountingarm154 can be configured to support, hold and/or positionrotary evaporator assembly140 such thatrotary evaporator assembly140 is an integrated component, or can become an integrated component by mounting to mountingarm154, ofdistillation apparatus102, along withchiller120 andcondenser180. In someembodiments mounting arm154 can be mechanically linked tomain housing132 by a verticallyadjustable member162 that is configured to allow mountingarm154, and attachedrotary evaporator assembly140, to raise and lower vertically as need to optimally position the sample flask in a water bath. In some embodiments verticallyadjustable member162 can comprise a motorized member configured to move mountingarm154 alongtrack160 or other guiding component to thereby raise and lower mountingarm154. The track or guiding component of verticallyadjustable member162 can in some embodiments be integrated into a portion of the main frame or housing of the chiller, such as for examplemain housing132.
• Rotaryevaporator assembly140 can comprise a rotary joint (vapor duct)150 with asample flask142 at one end, wherebysample flask142 can be rotated integrally with rotary joint150.Sample flask142 can be soaked, bathed or immersed withinwater bath156, in some embodiments a heated water bath to cause evaporation of the sample or solvent insample flask142.Water bath156 can comprise a heating element and controller or other configuration for heating water or other liquid/fluid contained therein.Sample flask142 can be connected to one end of rotary joint150 through a vapor duct that can be insertedly supported by a rotor of a motor through a sleeve housed within mountingarm154. Vapor duct/rotary joint150 can act both as the axis for sample rotation, and as vacuum-tight conduit for the vapor being drawn off of the sample. On the other side of rotary joint150 there can in some embodiments be one or more condensers (condenser180 and/or dummy condenser144) connected byvapor duct150 to receive and thereby condense vapors evaporated fromsample flask142. In someembodiments dummy condenser144 can be used, and can comprise anupper portion146 andlower portion148.
• Continuing withFIG. 1B, an evaporating (sample) flask142 can be immersed in awater bath156. Evaporatingflask142 can be rotated using a motor housed in mountingarm154, with the rotational force provided by the motor being transferred to evaporatingflask142 by rotary joint (vapor duct)150. Rotary joint150 can pass/continue through mountingarm154. Together, rotary joint (vapor duct)150 can provide a conduit through which the evaporate (vapor) from a sample or solvent inevaporation flask142 can pass into acondenser180 attached to or in communication with vapor duct150 (illustrated inFIG. 4). Once incondenser180 vapors can be cooled thereby causing them to re-condense and drop intocollection flask186. After the solvent has been removed (by evaporation), evaporatingflask142 can be removed fromwater bath156 by raising mountingarm154 by way of verticallyadjustable member162, which in some embodiments can comprise a track and motor or other mechanized unit.
• Continuing withFIG. 1B,water bath156 can be arranged in front ofmain housing132. Such a configuration can minimize the footprint ofdistillation apparatus100, particularly as compared to a distillation system where a water bath is not integrated and is instead placed or arranged on a surface adjacent to the distillation apparatus. Moreover, mountingarm154 arranged onmain housing132 and being vertically adjustable allows forrotary evaporating assembly140 to be raised and lowered such thatsample flask142 can be placed into or removed fromwater bath156 without having to movewater bath156. By vertically orienting these components the overall footprint of the all-in-oneintegrated distillation apparatus102 is greatly reduced, particularly as compared to non-integrated systems.
• Condenser180 can be attached tocondenser arm134 byclamp196, or other attachment mechanism, e.g. threads, screws, bolts, pressure fitting, etc.Condenser180 is otherwise the same in the embodiment illustrated inFIG. 1B as in the embodiment illustrated inFIG. 1A.
• FIGS. 2A through 2E illustrate the condenser apparatus that can in some embodiments be used in one or more embodiments of the disclosed distillation apparatuses.FIG. 2A depictscondenser coil182, made from a copper tubing material in some embodiments, or alternatively stainless steel, other suitable metal alloys such as titanium. In someembodiments condenser coil182 can comprise a titanium material with an inner coating of copper.Condenser coil182 can have anincoming line202 for receiving a flow of chilled coolant or refrigerant to pass through the coils, and anoutgoing line204 configured as a conduit for the outgoing coolant or refrigerant after having passed through the coils and acting as a heat exchanger.Incoming line202 andoutgoing line204 are configured to be connected to the integrated refrigeration system ofchiller120.Condenser coil182 can in some embodiments be double looped to increase the surface area for cooling and heat exchange.
• FIG. 2B depictscondenser sleeve198 that can comprise a chemically-resistant material such as but not limited to titanium (including commercial pure grade titanium), stainless steel, metal alloys, plastic, glass, rubber, such as neoprene rubber, and/or combinations thereof. In some embodiments titanium is used in the sleeve due to its robust chemical resistance. In some embodiments condensersleeve198 can comprise a titanium tubular structure with an enclosed lower end and openupper end212, and having a diameter sufficient to receive or slidingly engagecondenser coil182 as depicted inFIG. 2D.Condenser sleeve198 can comprise acollar210 having a larger diameter than the tubular structure ofcondenser sleeve198, and can in some embodiments be configured to mechanically engage, e.g. by threads, pins, slots, screws and/or other attachment/securement mechanisms tocondenser arm124,134.
• FIG. 2C illustrates an embodiment of acondenser housing184, comprising in some embodiments a glass vessel configured to enclose or otherwise surround a heat exchanger that includescondenser coil182 andcondenser sleeve198.Condenser housing184 can attach tocondenser arm124,134 by a clamp or other securing mechanism to create an air-tight seal, and in some embodiments can abutcollar210 ofcondenser sleeve198.Condenser housing184 can comprise a substantially cylindrical glass sleeve of a sufficient diameter to receivecondenser sleeve198 and/orcondenser coil182 in on upperopen end214.
• Condenser housing184 can comprise anentry port188 for receiving an evaporate or vapor from rotary evaporator assembly, and in some embodiments asecond entry port188′. Avacuum port190 can in some embodiments be provided (in some cases near the top) and configured to receive a vacuum line from a vacuum pump to thereby cause a vacuum on the inner environment ofcondenser housing184. An evaporate or vapor that comes into contact withheat exchanger198 incondenser180 and thereby condenses into a liquid can collect intocollection flask186 by passing throughconduit158. In some embodiments a joint192 can be positioned onconduit158 that can be configured to allow for removal of a collection flask (receiving flask)186 without breaking a vacuum to the system during operation. Such joint192 can comprise a valve to maintain the vacuum while removingcollection flask186.
• FIG. 2D illustrates a cut-away view ofcondenser sleeve198 withcondenser coil182 residing therein to form a heat exchanger or “cold finger”. Similarly,FIG. 2E illustratescondenser housing184 withcondenser sleeve198 residing therein (noteincoming line202 andoutgoing line204 ofcondenser coil182 extending above opening212 ofcondenser sleeve198 indicating the presence ofcondenser coil182 insidecondenser sleeve198.).
• FIG. 3 is a cross-sectional view of an distillation apparatus as disclosed herein. For illustration purposes onlyFIG. 3 most closely resembles a cross-sectional view of the embodiment depicted inFIG. 1B, but the components of the refrigeration system and condenser system depicted inFIG. 3 is equally applicable to other embodiments and configurations. As illustrated inFIG. 3distillation apparatus102 can comprisechiller120 andcondenser180 connected bycondenser arm134.Condenser coil182 insidecondenser sleeve198 forms a continuous loop with the refrigeration system inchiller120 by way ofconduit408. In someembodiment conduit408 comprises a copper tubing that facilitates the fluid flow of a cooling agent or refrigerant compound through the refrigeration system, intocondenser coil182, together withcondenser sleeve198 acting as a heat exchanger, and back through the refrigeration system in a continuous loop. The refrigeration system can comprise areceiving tank404,compressor402,refrigeration condenser400 anddryer406. All, or substantially all, of the components of the refrigeration system can be housed insidemain housing132 ofchiller120.
• FIG. 4 is a perspective view of a distillation apparatus with an integrated rotary evaporator assembly connected to a condenser. Particularly,distillation apparatus100 is similar to that disclosed inFIG. 1A but with the addition of connections, e.g. tubing, between rotaryevaporator assembly140condenser180. In thisembodiment dummy condenser144 can be connected tocondenser180 bytubing240,242. Particularly, in some embodimentsupper portion146 can be connected toinlet188′ viaoutlet332, whilelower portion148 can be connected toinlet188 via outlet/conduit336, or vice versa. In some embodimentslower portion148 ofdummy condenser144 can comprise an outlet or port comprising avalve244 that can be closed when not connected viatubing242. Thus, in some embodiments onlyupper portion146 can be connected tocondenser180 bytubing240 at eitherinlet188 or188′. Alternatively, bothtubing240 and242 can connect to a single inlet, either188 or188′.
• Tubing240 and242 can be a flexible tubing material that allowsrotary evaporator assembly140 to be connected tocondenser180 all the while allowing for rotaryevaporator assembly140 to be moved up and down as needed to submerge or removesample flask142 inwater bath156 without having to disconnectcondenser180. By usingdummy condenser144 such a configuration allows for free movement and adjustment ofrotary evaporator assembly140 in the integrated distillation apparatus. Such advantages are not afforded by other systems.
• Moreover, in someembodiments vacuum line246 can connect a vacuum system or pump (not shown) tovacuum port190. In some embodiments vacuum system or pump can be integrated withinhousing122, for example, or can be a stand alone separate unit.
• FIG. 5 is a schematic500 illustrating the flow or transfer of heat energy with a distillation apparatus as disclosed herein, including for example from a rotary evaporator assembly to a chiller or cooling system. In afirst step1 heat from a rotary evaporator assembly can be captured by a condenser/heat exchanger502 and directed through areceiver tank504 andcompressor506 via a refrigerant compound. In asecond step2 the heat can be removed from the refrigerant compound byrefrigeration condenser508. In athird step3 the cooled refrigerant compound can pass through adryer510 and then in a fourth step4 can be recirculated back to condenser/heat exchanger502 to capture heat generated by the rotary evaporator. The integrated design of the disclosed distillation apparatuses provides for this efficient transfer of heat energy from the rotary evaporator system to the refrigeration system (cooling system) in a self-contained and compact system.
• FIGS. 6A and 6B illustrate alternative embodiments of distillation apparatuses disclosed herein.Distillation apparatuses104 and106 are similar todistillation apparatus100 illustrated inFIG. 1A, but with different configurations forwater bath250. Note that rotary evaporator assemblies are not shown inFIGS. 6A and 6B for simplicity, but can be attached and incorporated as described herein and shown in the figures, e.g.FIG. 1A.
• InFIG.6A water bath250 is positioned on an upper side oflower housing122 and resting on aplatform252.Platform252 can be configured to move in a horizontal direction to translate the position ofwater bath250 as needed to align with a rotary evaporator. Alternatively, or in addition,platform252 can be configured to move in a vertical direction, and/or vertical and horizontal direction, to translate the position ofwater bath250 as needed to align with a rotary evaporator.
• InFIG.6B water bath250 is positioned in front of or on a front portion oflower housing122 and resting on aplatform252.Platform252 can be configured to move in a vertical direction to raise and lower the position ofwater bath250 as needed to align with a rotary evaporator. Alternatively, or in addition,platform252 can be configured to move in a horizontal direction, and/or vertical and horizontal direction, to translate the position ofwater bath250 as needed to align with a rotary evaporator.
• FIGS. 7A and 7B illustrate embodiments of distillation apparatuses disclosed herein. Thedistillation apparatuses108 and110 inFIGS. 7A and 7B, respectively, are analogous todistillation apparatuses100 and102, respectively, with exception to the fixed condenser arms and dummy condenser. In the designs illustrated inFIGS. 7A and 7B fixed condenser arms (seecondenser arms124 and134 inFIGS. 1A and 1B, respectively) are replaced withflexible coolant lines248. Moreover, nodummy condenser144 is needed in the configurations illustrated inFIGS. 7A and 7B.
• To elaborate, as depicted inFIGS. 7A and 7B, fully integrated all-in-onedistillation apparatus108 and110, respectively, can comprise achiller120, arotary evaporator assembly140 and acondenser180. In some embodiments, and as shown inFIGS. 1A and 1B, thechiller120,rotary evaporator assembly140, and acondenser180, can be integrated into a single device or apparatus that is configured to compactly arrange the elements in such a way that provides for an effective and efficient distillation system while minimizing the operational area and/or footprint.
• Continuing withFIG. 7A,distillation apparatus100 can comprise achiller120.Chiller120 can comprise in some embodiments alower housing122 andupper housing126, withupper housing126 extending substantially vertically fromlower housing122. In someembodiments chiller120 can comprise aflexible coolant line248 extending fromupper housing126 fluidly connectingcondenser180 tochiller120.Chiller120 can comprise an integrated refrigeration system (seeFIG. 3) housed withinlower housing122 andupper housing126, and continuing throughflexible coolant line248 to provide a cooled refrigerant tocool condenser180. In some embodiments,lower housing122 can house components of a refrigeration system (solely or in conjunction with upper housing126), such as for example a receiving tank, compressor, refrigeration condenser and dryer (seeFIG. 3), all or some of which can bee connected by refrigeration lines (copper tubing) tocondenser180 by feeding throughupper housing126 andflexible coolant line248. In some embodimentslower housing122 can comprise ventilation grates194 configured to allow airflow intohousing122 and around the refrigeration system housed therein.
• Mountingarm154 can be mechanically linked to and can extend (substantially horizontally in some embodiments) fromupper housing126. Mountingarm154 can be configured to support, hold and/or positionrotary evaporator assembly140 such thatrotary evaporator assembly140 is an integrated component, or can become an integrated component by mounting to mountingarm154, ofdistillation apparatus100, along withchiller120 andcondenser180. In someembodiments mounting arm154 can be mechanically linked toupper housing126 by a verticallyadjustable member160 that is configured to allow mountingarm154, and attachedrotary evaporator assembly140, to raise and lower vertically as need to optimally position the sample flask in a water bath. In some embodiments verticallyadjustable member160 can comprise a motorized member configured to move mountingarm154 along a track or other guiding component to thereby raise and lower mountingarm154. The track or guiding component of verticallyadjustable member160 can in some embodiments be integrated into a portion of the main frame or housing of the chiller, such as for exampleupper housing126.
• Rotaryevaporator assembly140 can comprise a rotary joint (vapor duct)150 with asample flask142 at one end, wherebysample flask142 can be rotated integrally with rotary joint150.Sample flask142 can be soaked, bathed or immersed withinwater bath156, in some embodiments a heated water bath to cause evaporation of the sample or solvent insample flask142.Water bath156 can comprise a heating element and controller or other configuration for heating water or other liquid/fluid contained therein.Sample flask142 can be connected to one end of rotary joint150 through a vapor duct that can be insertedly supported by a rotor of a motor through a sleeve housed within mountingarm154. Vapor duct/rotary joint150 can act both as the axis for sample rotation, and as vacuum-tight conduit for the vapor being drawn off of the sample. On the other side of rotary joint150 there can in some embodiments condenser180 connected byvapor duct150 to receive and thereby condense vapors evaporated fromsample flask142.
• Continuing withFIG. 7A, an evaporating (sample) flask142 can be immersed in awater bath156. Evaporatingflask142 can be rotated using a motor housed in mountingarm154, with the rotational force provided by the motor being transferred to evaporatingflask142 by rotary joint (vapor duct)150. Rotary joint150 can pass/continue through mountingarm154. Together, rotary joint150 can provide a conduit through which the evaporate (vapor) from a sample or solvent inevaporation flask142 can pass into acondenser180 attached to or in communication withvapor duct150. Once incondenser180 vapors can be cooled thereby causing them to re-condense and drop intocollection flask186. After the solvent has been removed (by evaporation), evaporatingflask142 can be removed fromwater bath156 by raising mountingarm154 by way of verticallyadjustable member160, which in some embodiments can comprise a track and motor or other mechanized unit.
• Continuing withFIG. 7A,water bath156 can be arranged on top oflower housing122 and adjacent toupper housing126. Such a configuration can minimize the footprint ofdistillation apparatus100, particularly as compared to a distillation system where a water bath is not integrated and is instead placed or arranged on a surface adjacent to the distillation apparatus. Moreover, mountingarm154 arranged onupper housing126 and being vertically adjustable allows forrotary evaporating assembly140 to be raised and lowered such thatsample flask142 can be placed into or removed fromwater bath156 without having to movewater bath156. By vertically orienting these components the overall footprint of the all-in-oneintegrated distillation apparatus100 is greatly reduced, particularly as compared to non-integrated systems.
• All components ofcondenser180 can be similar to that already described with respect toFIG. 1A.
• Turning now to theFIG. 7B,distillation apparatus102 can comprise achiller120.Chiller120 can comprise in some embodiments amain housing132, optionally supported onplatform170. In someembodiments chiller120 can comprise aflexible coolant line248 extending frommain housing132 and configured to fluidly connectcondenser180 tochiller120.Chiller120 can comprise an integrated refrigeration system (seeFIG. 3) housed withinmain housing132 and continuing throughflexible coolant line248 to provide a cooled refrigerant tocool condenser180. In some embodiments,main housing132 can house components of a refrigeration system (solely or in conjunction with condenser arm134), such as for example a receiving tank, compressor, refrigeration condenser and dryer (seeFIG. 3), all or some of which can bee connected by refrigeration lines (copper tubing) tocondenser180 by feeding throughflexible coolant line248. In some embodimentsmain housing132 can comprise ventilation grates194 configured to allow airflow intohousing132 and around the refrigeration system housed therein.
• Mountingarm154 can be mechanically linked to and can extend (substantially horizontally in some embodiments) frommain housing132. Mountingarm154 can be configured to support, hold and/or positionrotary evaporator assembly140 such thatrotary evaporator assembly140 is an integrated component, or can become an integrated component by mounting to mountingarm154, ofdistillation apparatus102, along withchiller120 andcondenser180. In someembodiments mounting arm154 can be mechanically linked tomain housing132 by a verticallyadjustable member162 that is configured to allow mountingarm154, and attachedrotary evaporator assembly140, to raise and lower vertically as need to optimally position the sample flask in a water bath. In some embodiments verticallyadjustable member162 can comprise a motorized member configured to move mountingarm154 alongtrack160 or other guiding component to thereby raise and lower mountingarm154. The track or guiding component of verticallyadjustable member162 can in some embodiments be integrated into a portion of the main frame or housing of the chiller, such as for examplemain housing132.
• Rotaryevaporator assembly140 can comprise a rotary joint (vapor duct)150 with asample flask142 at one end, wherebysample flask142 can be rotated integrally with rotary joint150.Sample flask142 can be soaked, bathed or immersed withinwater bath156, in some embodiments a heated water bath to cause evaporation of the sample or solvent insample flask142.Water bath156 can comprise a heating element and controller or other configuration for heating water or other liquid/fluid contained therein.Sample flask142 can be connected to one end of rotary joint150 through a vapor duct that can be insertedly supported by a rotor of a motor through a sleeve housed within mountingarm154. Vapor duct/rotary joint150 can act both as the axis for sample rotation, and as vacuum-tight conduit for the vapor being drawn off of the sample. On the other side of rotary joint150 there can in some embodiments be condenser180 connected byvapor duct150 to receive and thereby condense vapors evaporated fromsample flask142.
• Continuing withFIG. 7B, an evaporating (sample) flask142 can be immersed in awater bath156. Evaporatingflask142 can be rotated using a motor housed in mountingarm154, with the rotational force provided by the motor being transferred to evaporatingflask142 by rotary joint (vapor duct)150. Rotary joint150 can pass/continue through mountingarm154. Together, rotary joint150 can provide a conduit through which the evaporate (vapor) from a sample or solvent inevaporation flask142 can pass into acondenser180 attached to or in communication with vapor duct150 (illustrated inFIG. 4). Once incondenser180 vapors can be cooled thereby causing them to re-condense and drop intocollection flask186. After the solvent has been removed (by evaporation), evaporatingflask142 can be removed fromwater bath156 by raising mountingarm154 by way of verticallyadjustable member162, which in some embodiments can comprise a track and motor or other mechanized unit.
• Continuing withFIG. 7B,water bath156 can be arranged in front ofmain housing132. Such a configuration can minimize the footprint ofdistillation apparatus110, particularly as compared to a distillation system where a water bath is not integrated and is instead placed or arranged on a surface adjacent to the distillation apparatus. Moreover, mountingarm154 arranged onmain housing132 and being vertically adjustable allows forrotary evaporating assembly140 to be raised and lowered such thatsample flask142 can be placed into or removed fromwater bath156 without having to movewater bath156. By vertically orienting these components the overall footprint of the all-in-oneintegrated distillation apparatus102 is greatly reduced, particularly as compared to non-integrated systems.
• Condenser180 is otherwise the same in the embodiment illustrated inFIG. 7B as in the embodiment illustrated inFIG. 7A.
• In bothFIGS. 7A and7B vapor duct150 can be directly connected tocondenser180, and particularlycondenser housing184. As such,rotary evaporating assembly140 is directly connected tocondenser180 without the use of a dummy condenser. Thus, when mountingarm154 moves vertically to raise or lowerrotary evaporating assembly140condenser180 correspondingly moves.Flexible coolant line248 allows for such movement while maintaining fluid communication with the refrigeration system inchiller120.
• FIGS. 8A and 8B illustrate additional embodiments ofdistillation apparatuses112 and114, respectively. As depicted inFIGS. 8A and 8B, fully integrated all-in-onedistillation apparatus112 and114, respectively, can comprise achiller120, arotary evaporator assembly140 and acondenser180. In some embodiments, and as shown inFIGS. 8A and 8B, thechiller120,rotary evaporator assembly140, and acondenser180, can be integrated into a single device or apparatus that is configured to compactly arrange the elements in such a way that provides for an effective and efficient distillation system while minimizing the operational area and/or footprint.
• Continuing withFIG. 8A,distillation apparatus112 can comprise achiller120.Chiller120 can comprise in some embodiments alower housing122 andupper housing304, withupper housing304 extending substantially vertically fromlower housing122. In someembodiments chiller120 can comprise acondenser arm124 extending substantially horizontally fromupper housing304 and configured to support and mechanically connectcondenser180 tochiller120.Chiller120 can comprise an integrated refrigeration system (seeFIG. 3) housed withinlower housing122 andupper housing304, and continuing throughcondenser arm124 to provide a cooled refrigerant tocool condenser180. In some embodiments,lower housing122 can house components of a refrigeration system (solely or in conjunction with upper housing304), such as for example a receiving tank, compressor, refrigeration condenser and dryer (seeFIG. 3), all or some of which can bee connected by refrigeration lines (copper tubing) tocondenser180 by feeding throughupper housing304 andcondenser arm124. In some embodimentslower housing122 can comprise ventilation grates194 configured to allow airflow intohousing122 and around the refrigeration system housed therein.
• Mountingarm154 can be mechanically linked to and can extend (substantially horizontally in some embodiments) fromupper housing304. Mountingarm154 is otherwise similar to that described above with respect toFIG. 1A. Moreover,rotary evaporator assembly140 andcondenser180 inFIG. 8A is similar to that described above with respect toFIG. 1A.
• Turning now to theFIG. 8B,distillation apparatus114 can comprise achiller120.Chiller120 can comprise in some embodiments amain housing132, optionally supported onplatform170, andupper housing302. In someembodiments chiller120 can comprise acondenser arm134 extending substantially horizontally fromupper housing302, in some embodiments from an upper portion ofupper housing302, and configured to support and mechanically connectcondenser180 tochiller120.Chiller120 can comprise an integrated refrigeration system (seeFIG. 3) housed withinmain housing132 and continuing throughcondenser arm124 to provide a cooled refrigerant tocool condenser180. In some embodiments,main housing132 can house components of a refrigeration system (solely or in conjunction withcondenser arm134 and/or upper housing302), such as for example a receiving tank, compressor, refrigeration condenser and dryer (seeFIG. 3), all or some of which can bee connected by refrigeration lines (copper tubing) tocondenser180 by feeding throughcondenser arm134. In some embodimentsmain housing132 can comprise ventilation grates194 configured to allow airflow intohousing132 and around the refrigeration system housed therein.
• Mountingarm154 can be mechanically linked to and can extend (substantially horizontally in some embodiments) fromupper housing132. Mountingarm154 is otherwise similar to that described above with respect toFIG. 1B. Moreover,rotary evaporator assembly140 andcondenser180 inFIG. 8B is similar to that described above with respect toFIG. 1B.
• In the embodiments depicted inFIGS. 8A and 8B anaccordion element300 is provided.Accordion element300 can be configured to be placed between and joincondenser180, and specifically condenserhousing184, todummy condenser144. In such aconfiguration accordion element300 can be configured to be collapsible and/or expandable so as to allow for the vertical raising and lowering ofrotary evaporator assembly140 while maintaining a connection tocondenser180 that is in a fixed position. In some embodimentslower portion148 ofdummy condenser144 can function as a collection flask for the condensate.
• FIGS. 9A through 9C illustrate components of a rotary evaporator assembly as can be utilized with the disclosed distillation apparatuses.FIG. 9A is an exploded or component view of a rotary evaporator assembly. Rotary evaporator assembly can comprise a rotary joint (vapor duct)150 and amotor assembly320 configured to receive rotary joint (vapor duct)150 as depicted inFIG. 9B.Motor assembly320 is configured to be housed within or affixed to mountingassembly154 as show inFIGS. 1A and 1B for example. Rotary joint (vapor duct)150 can be insertedly supported by a rotor ofmotor assembly320 through a sleeve housed withinmotor assembly320. Vapor duct/rotary joint150 can act both as the axis for sample rotation, and as vacuum-tight conduit for the vapor being drawn off of the sample insample flask142.Sample flask142 can be connected to one end of rotary joint150, such as for example through opening324 (and in some embodiments secured by clip322), wherebysample flask142 can be rotated integrally with rotary joint150, as shown in assembled version inFIG. 9C. On the other end of rotary joint150 there can in some embodiments be one or more condensers (condenser180 and/ordummy condenser144 as shown inFIG. 9A) connected byvapor duct150 to receive and thereby condense vapors evaporated fromsample flask142. In someembodiments dummy condenser144 can be used, and can comprise anupper portion146 andlower portion148, as well as aconnector arm328 secured to mountingarm154 and/ormotor assembly320 and through which rotary joint150 passes intoupper portion146.Lip326, which can also comprise a fastener, can be configured to secureconnector arm328 to mountingarm154 and/ormotor assembly320. In some embodiments avacuum seal330 can be used to create an air-tight seat at this joint.Dummy condenser144 can comprise anoutlet332, conduit344 and outlet/conduit336.
• FIG. 10 is a perspective view of a distillation apparatus as disclosed herein, with a plurality of condensers. Particularly,distillation apparatus116 can be the same asdistillation apparatus102 inFIG. 1B, but with anadditional condenser180′.Condenser180′ can be secured bycondenser arm134′ just ascondenser180 can be secured bycondenser arm134.Condenser180′ can in some embodiments function similarly tocondenser180, and can provide additional cooling capacity for use in condensing evaporates from a rotary evaporator, or other uses in a laboratory where cooling is required.Condenser180′ can be in fluid communication with the mechanical refrigeration system just ascondenser180.
• Condenser180′ can be attached tocondenser arm134′ byclamp196′, or other attachment mechanism, e.g. threads, screws, bolts, pressure fitting, etc.Condenser180′ can comprisecondenser coil182′,condenser sleeve198′ andcondenser housing184′.Condenser coil182′ can be configured to fit or slide insidecondenser sleeve198′ to form a heat exchanger or “cold finger”.Condenser coil182′ can in some embodiments be double looped to increase the surface area for cooling and heat exchange.Condenser coil182′ can be fluidly connected to the integrated refrigeration system inchiller120 such that cooled refrigerant passing throughcondenser coil182′ causes a cooling effect oncondenser sleeve198′. Evaporate or vapor fromrotary evaporator140 enteringcondenser housing184′ can come into contact with the cold surface ofcondenser sleeve198′ thereby causing the vapor to condense into a liquid to be collected incollection flask186′. The configuration ofcondenser180′ provides an efficient mechanism for trapping all or substantially all vapors and condensing them such that environmental impacts are lessened.
• In someembodiments condenser coil182′ can comprise coiled copper line that forms a continuous loop thereby providing for a continuous flow of a refrigerant material or compound to flow from the heat exchanger incondenser180′ to the mechanical refrigeration system inchiller120. While in someembodiments condenser coil182′ can be exposed for direct cooling of evaporate (vapor), as depicted inFIG. 10 it can be concealed bycondenser sleeve198′ that can comprise a chemically-resistant vapor trap made of titanium (including commercial pure grade titanium), stainless steel, metal alloys, plastic, glass, rubber, such as neoprene rubber, and/or combinations thereof. As depicted inFIG. 10, and in order to achieve a stand alone fully integrated system that minimizes space utilization,chiller120, including mechanical refrigeration system, can be mechanically linked to and fixed with the heat exchanger/condenser180′ such that the two are provided in a single unitary device.
• Condenser housing184′ can comprise a glass vessel enclosing the heat exchanger that includescondenser coil182′ andcondenser sleeve198′.Condenser housing184 can attach tocondenser arm134′ byclamp196′ to create an air-tight seal.Condenser housing184′ can comprise anentry port188′ for receiving an evaporate or vapor fromrotary evaporator assembly140, and in some embodiments a second (or more)entry port188″. Avacuum port190′ can in some embodiments be provided (in some cases near the top) and configured to receive a vacuum line from a vacuum pump to thereby cause a vacuum on the inner environment ofcondenser housing184′. An evaporate or vapor that comes into contact withheat exchanger198′ incondenser180′ and thereby condenses into a liquid can collect intocollection flask186′ by passing throughconduit158′. In some embodiments a joint192′ can be positioned onconduit158′ that can be configured to allow for removal of a collection flask (receiving flask)186′ without breaking a vacuum to the system during operation. Such joint192′ can comprise a valve to maintain the vacuum while removingcollection flask186′.
• Although only shown with one embodiment of the distillation apparatus (FIG. 1B/FIG. 10), the double or plurality of condensers can be applied to all configurations/embodiments of distillation apparatuses disclosed herein, including but not limited to those illustrated inFIGS. 1A, 1B, 3, 4, 6A, 6B, 7A, 7B, 8A and 8B.
• In some embodiments, a disclosed distillation apparatus can further comprises a system vacuum valve that can be configured to allow for removal of a receiving flask without breaking a vacuum to the system during operation.
• In some aspects, the rotation can be synced with heating, i.e. the heating bath can turned on when rotation starts and goes into standby mode when rotation stops. Such a configuration can save energy and water.
• In some embodiments, a cooling temperature range can be from ambient to about −150° C., or about −20° C. to about −100° C. Desired temperatures achieved through refrigeration engineering and refrigerant selection can achieve such ultra-low ranges.
• In some embodiments, a distillation apparatus can comprise a vacuum seal inside the condenser, which can provide an internal vacuum seal to further guard against vacuum leak commonly associated with conventional rotary evaporators. Existing rotary evaporators have the vacuum seal located where the condenser attaches to the rotating unit. Disclosed herein is an evaporator with the vacuum seal inside the cooling unit. In such a configuration the O-ring can be accessible from inside the cooling unit. The cooling unit can be fused to the rotating unit. The O-ring can be incorporated from inside the cooling unit. This can remove the joint between the traditional condenser and the rotating unit, with the benefit of eliminating a potential vacuum leak at the joint. An internally contained O-ring seal can provide that even in the event of a slight vacuum leak there will no drop in vacuum.
• The seals that connect the condenser unit with the rotating motor in existing models are not as robust as they could be. In some embodiments provided herein there are fewer joints in general to reduce the sources of leaks. In some embodiments, a rotary evaporator is provided with substantially 100% proof vacuum seal between the condenser unit and rotating unit.
• It can be desirable to provide distillation apparatuses and systems that have a footprint or operational area that is a small as possible. That is, given the sometimes limited space in a laboratory or research facility equipment that takes up as little space as possible can be highly desirable. Thus, in some aspects the instant disclosure provides distillation apparatuses and systems that have a substantially reduced or smaller footprint that takes up less space than conventional distillation apparatuses and systems. Such compact designs are made possible by the unique configurations and integrations of components. In some embodiments, the footprint or operational area of a distillation apparatus can be defined by the length L, width W, and/or combination thereof (area in square inches for example) of the outer dimensions of the apparatus. Alternatively, or in addition, the footprint or operational area of a distillation apparatus can be defined by the length X, width Y, and/or combination thereof (area in square inches for example) of the dimensions of the base or platform of the housing/frame.
• By way of example and not limitation, the footprint of traditional or existing rotary evaporators is about 300 to about 500 square inches, with some designs having an about 368 square inch footprint. In contrast, the presently disclosed distillation apparatuses, including chiller, condenser and rotary evaporator, can in some embodiments comprise a total footprint of about 150 square inches to about 350 square inches. For example, where the heating bath located in front of the base or housing the total footprint can be about 350 square inches (base 230 square inches andheating bath 120 square inches). In some aspects, particularly where the compact design includes a heating bath on top of the base or housing, the footprint of the heating bath is removed. Thus, the total footprint of a compact design of a disclosed distillation apparatus can be about 150 square inches to about 230 square inches.
• In some embodiments, the rotary stand and heating or water bath can be mounted on top of the chiller housing. Such a configuration can significantly decrease the overall footprint of the unit. The more compact design can take advantage of a shorter refrigeration compressor height, such as for example about 6 inches, about 8 inches, or about 10 inches, which in turn provides sufficient space for the heating bath to be positioned above the compressor (housed inside the chiller housing) and the rotating stand above the condenser. In some aspects, a refrigeration condenser can have a height of about 8 inches, or about 10 inches, or about 12 inches.
• In some embodiments, including the compact design disclosed herein, the heating bath can move horizontally. Likewise, in some aspects the rotating stand can move vertically. Other components, such as the cooling coil, the electric switch board, and/or the receiving can be optimally positioned to allow for a reduced footprint. The electronic control unit, for example, can be ergonomically located in front of the housing of the chiller.
• While the following terms are believed to be well understood by one of ordinary skill in the art, the following definitions are set forth to facilitate explanation of the presently disclosed subject matter.
• Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood to one of ordinary skill in the art to which the presently disclosed subject matter belongs. Although any methods, devices, and materials similar or equivalent to those described herein can be used in the practice or testing of the presently disclosed subject matter, representative methods, devices, and materials are now described.
• Following long-standing patent law convention, the terms “a”, “an”, and “the” refer to “one or more” when used in this application, including the claims. Thus, for example, reference to “a cell” includes a plurality of such cells, and so forth.
• Unless otherwise indicated, all numbers expressing quantities of ingredients, reaction conditions, and so forth used in the specification and claims are to be understood as being modified in all instances by the term “about”. Accordingly, unless indicated to the contrary, the numerical parameters set forth in this specification and attached claims are approximations that can vary depending upon the desired properties sought to be obtained by the presently disclosed subject matter.
• As used herein, the term “about,” when referring to a value or to an amount of a composition, dose, sequence identity (e.g., when comparing two or more nucleotide or amino acid sequences), mass, weight, temperature, time, volume, concentration, percentage, etc., is meant to encompass variations of in some embodiments ±20%, in some embodiments ±10%, in some embodiments ±5%, in some embodiments ±1%, in some embodiments ±0.5%, and in some embodiments ±0.1% from the specified amount, as such variations are appropriate to perform the disclosed methods or employ the disclosed compositions.
• The term “comprising”, which is synonymous with “including” “containing” or “characterized by” is inclusive or open-ended and does not exclude additional, unrecited elements or method steps. “Comprising” is a term of art used in claim language which means that the named elements are essential, but other elements can be added and still form a construct within the scope of the claim.
• As used herein, the phrase “consisting of” excludes any element, step, or ingredient not specified in the claim. When the phrase “consists of” appears in a clause of the body of a claim, rather than immediately following the preamble, it limits only the element set forth in that clause; other elements are not excluded from the claim as a whole.
• As used herein, the phrase “consisting essentially of” limits the scope of a claim to the specified materials or steps, plus those that do not materially affect the basic and novel characteristic(s) of the claimed subject matter.
• With respect to the terms “comprising”, “consisting of”, and “consisting essentially of”, where one of these three terms is used herein, the presently disclosed and claimed subject matter can include the use of either of the other two terms.
• As used herein, the term “and/or” when used in the context of a listing of entities, refers to the entities being present singly or in combination. Thus, for example, the phrase “A, B, C, and/or D” includes A, B, C, and D individually, but also includes any and all combinations and subcombinations of A, B, C, and D.
• It will be understood that various details of the presently disclosed subject matter may be changed without departing from the scope of the presently disclosed subject matter. Furthermore, the foregoing description is for the purpose of illustration only, and not for the purpose of limitation.

Claims (27)

1. An integrated distillation apparatus, comprising:

a rotary evaporator configured to evaporate a sample;

a condenser configured to condense an evaporated sample;

a refrigeration system configured to cool the condenser;

a collection vessel configured to collect a condensate; and

a vacuum pump configured to create a vacuum in the evaporator, wherein each of the components is integrated into a single apparatus.

2. The integrated distillation apparatus ofclaim 1, further comprising:

a motorized component configured to provide a rotational force;

a rotary joint insertedly supported within the motorized component upon which the rotational force is applied;

a sample container connected to a first end of the rotary joint;

a water bath into which the sample container can be placed, wherein the water bath is configured to provide heat energy to the sample container;

a condenser connected to a second end of the rotary joint, wherein the condenser is configured to receive a collection flask that receives condensed vapors condensed off of the condenser; and

a cooling coil configured to engage the condenser, wherein the cooling coil is configured to receive coolant from the refrigeration system, whereby the condenser is sufficiently cool to condense vapors coming into contact with the condenser.

3. The integrated distillation apparatus ofclaim 2, further comprising a mechanical linkage configured to move the water bath in a vertical and/or horizontal direction to engage the sample container.

4. The integrated distillation apparatus ofclaim 2, wherein the refrigeration system comprises a condenser and refrigerant, wherein the refrigeration system provides coolant to the condenser to thereby condense vapors from the evaporator.

5. The integrated distillation apparatus ofclaim 4, wherein the coolant is provided to a double coil inside the condenser, wherein the vapors come into contact with the double coil or a wall surrounding the double coil.

6. The integrated distillation apparatus ofclaim 2, further comprising a frame configured to integrate all components into a single apparatus, wherein the water bath is configured to move relative to the rotary evaporator, wherein the rotary evaporator, refrigeration system, collection vessel, condenser and vacuum pump are stationary within the frame.

7. The integrated distillation apparatus ofclaim 2, wherein the collection vessel comprises a first and second compartment divided by a vacuum valve, wherein the first compartment can be removed to collect the condensate while the vacuum valve preserves the vacuum on the evaporator and the second compartment continues to collect condensate.

8. The integrated distillation apparatus ofclaim 2, wherein the condenser comprises two or more condensers in a series.

9. The integrated distillation apparatus ofclaim 2, further comprising a vacuum seal inside the condenser.

10. The integrated distillation apparatus ofclaim 9, wherein the vacuum seal inside the condenser comprises an O-ring incorporated inside the condenser at a point where the rotary evaporator engages the condenser.

11. The integrated distillation apparatus ofclaim 10, wherein the O-ring provides an internal vacuum seal.

12. The integrated distillation apparatus ofclaim 2, wherein the refrigeration system is configured to cool the condenser from about ambient temperature to about −100° C.

13. The integrated distillation apparatus ofclaim 2, wherein the integrated components are arranged such that a footprint of the integrated distillation apparatus is less than about 300 square inches.

14. The integrated rotary evaporator ofclaim 2, wherein the motorized component configured to provide a rotational force comprises a mechanical linkage configured to vertically move the rotary evaporator.

15. The integrated distillation apparatus ofclaim 2, wherein the condenser comprises a sleeve surrounding a cooling coil, wherein the sleeve comprises titanium material.

16. The integrated distillation apparatus ofclaim 2, further comprising a collapsible member disposed between the condenser and rotary evaporator, whereby the collapsible member is configured to allow an adjustment in the positioning of the rotary evaporator while connected to the condenser.

17. The integrated distillation apparatus ofclaim 1, further comprising a frame structure configured to house the refrigeration system and vacuum pump, and structurally support the rotary evaporator and condenser.

18. The integrated distillation apparatus ofclaim 17, wherein the frame structure is configured to support the condenser in a fixed position while supporting the rotary evaporator in a movable position.

19. An integrated distillation apparatus, comprising:

a rotary evaporator configured to evaporate a sample;

a condenser configured to condense an evaporated sample; and

a refrigeration system configured to cool the condenser, wherein the rotary evaporator, condenser and refrigeration system are integrated into a single structure,

wherein the rotary evaporator is movably attached to the structure and configured to be vertically translatable in position,

wherein the condenser is affixed to the structure by an arm extending from the structure and adjacent to the rotary evaporator, and

wherein the refrigeration system is in fluid communication with the condenser.

20. The integrated distillation apparatus ofclaim 19, further comprising a motorized component configured to provide a rotational force to the rotary evaporator.

21. The integrated distillation apparatus ofclaim 19, further comprising a mechanical linkage to vertically translate the position of the rotary evaporator.

22. The integrated distillation apparatus ofclaim 19, further comprising a heated water bath into which a sample container of the rotary evaporator can be submerged.

23. The integrated distillation apparatus ofclaim 19, wherein the condenser comprises a cooling coil in fluid communication with the refrigeration system.

24. The integrated distillation apparatus ofclaim 23, wherein the condenser comprises a titanium sleeve surrounding the cooling coil, whereby the titanium sleeve is cooled by the cooling coil, wherein an evaporate from the rotary evaporator comes into contact with the titanium sleeve and condenses.

25. The integrated distillation apparatus ofclaim 23, wherein the condenser comprises metal alloy sleeve surrounding the cooling coil, whereby the metal alloy sleeve is cooled by the cooling coil, wherein an evaporate from the rotary evaporator comes into contact with the metal alloy sleeve and condenses.

26. The integrated distillation apparatus ofclaim 19, wherein the refrigeration system comprises a compressor, refrigeration condenser, dryer and refrigerant.

27. The integrated distillation apparatus ofclaim 19, wherein the integrated apparatus comprises a footprint less than about 300 square inches.

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